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Isotope dilution-gas chromatography/mass spectrometry and liquid chromatography/electrospray ionization-tandem mass spectrometry for the determination of triiodo-L-thyronine in serum.
Rapid Commun Mass Spectrom. 1999; 13(19):1924-31.RC

Abstract

Isotope dilution-gas chromatography/mass spectrometry (ID-GC/MS) and isotope dilution-liquid chromatography/tandem mass spectrometry (ID-LC/MS/MS) methods have been developed for an determination of triiodothyronine (T3) in serum and their potential as candidate reference methods investigated. In both methods, (13)C(9)-T3 was used as internal standard. Sample pretreatment consisted of deproteinization, extraction and high performance liquid chromatography (HPLC) purification. Conversion of serum thyroxine (T4) to T3 was controlled by adding (13)C(6)-T4. For GC/MS, T3 and (13)C(9)-T3 were converted to the N,O-di-heptafluorobutyryl (HFB) methyl ester derivatives and monitored at m/z 844 and 853. For LC/MS with electrospray ionization, the transitions m/z 652/661 to 606/614 were monitored. For use of the methods as candidate reference methods, special attention was paid to the calibration and the measurement protocol (duplicate analysis of each sample on three occasions). Evaluation of the ID-GC/MS and ID-LC/MS/MS methods showed the absence of interference by reverse T3 and T4, a limit of detection of 100 pg (GC/MS) and 18 pg (LC/MS), a recovery of 100 +/- 1.5% (95% confidence interval) and good precision (the total coefficient of variation, n = 6, was typically 1.5%). In addition to the recovery study, the accuracy of the methods was proven by method comparison (ID-GC/MS vs. LC/MS/MS) on three sera, showing a maximum deviation of 1.1%. Finally, the ID-GC/MS method was applied for measurement of 10 different human sera with a T3 concentration range from 0.6 to 7.3 ng/mL.

Authors+Show Affiliations

Laboratorium voor Analytische Chemie, Faculteit Famaceutische Wetenschappen, Universiteit Gent Harelbekestraat 72, 9000 Gent, Belgium.No affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

10487939

Citation

Thienpont, L M., et al. "Isotope Dilution-gas Chromatography/mass Spectrometry and Liquid Chromatography/electrospray Ionization-tandem Mass Spectrometry for the Determination of triiodo-L-thyronine in Serum." Rapid Communications in Mass Spectrometry : RCM, vol. 13, no. 19, 1999, pp. 1924-31.
Thienpont LM, Fierens C, De Leenheer AP, et al. Isotope dilution-gas chromatography/mass spectrometry and liquid chromatography/electrospray ionization-tandem mass spectrometry for the determination of triiodo-L-thyronine in serum. Rapid Commun Mass Spectrom. 1999;13(19):1924-31.
Thienpont, L. M., Fierens, C., De Leenheer, A. P., & Przywara, L. (1999). Isotope dilution-gas chromatography/mass spectrometry and liquid chromatography/electrospray ionization-tandem mass spectrometry for the determination of triiodo-L-thyronine in serum. Rapid Communications in Mass Spectrometry : RCM, 13(19), 1924-31.
Thienpont LM, et al. Isotope Dilution-gas Chromatography/mass Spectrometry and Liquid Chromatography/electrospray Ionization-tandem Mass Spectrometry for the Determination of triiodo-L-thyronine in Serum. Rapid Commun Mass Spectrom. 1999;13(19):1924-31. PubMed PMID: 10487939.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Isotope dilution-gas chromatography/mass spectrometry and liquid chromatography/electrospray ionization-tandem mass spectrometry for the determination of triiodo-L-thyronine in serum. AU - Thienpont,L M, AU - Fierens,C, AU - De Leenheer,A P, AU - Przywara,L, PY - 1999/9/17/pubmed PY - 1999/9/17/medline PY - 1999/9/17/entrez SP - 1924 EP - 31 JF - Rapid communications in mass spectrometry : RCM JO - Rapid Commun Mass Spectrom VL - 13 IS - 19 N2 - Isotope dilution-gas chromatography/mass spectrometry (ID-GC/MS) and isotope dilution-liquid chromatography/tandem mass spectrometry (ID-LC/MS/MS) methods have been developed for an determination of triiodothyronine (T3) in serum and their potential as candidate reference methods investigated. In both methods, (13)C(9)-T3 was used as internal standard. Sample pretreatment consisted of deproteinization, extraction and high performance liquid chromatography (HPLC) purification. Conversion of serum thyroxine (T4) to T3 was controlled by adding (13)C(6)-T4. For GC/MS, T3 and (13)C(9)-T3 were converted to the N,O-di-heptafluorobutyryl (HFB) methyl ester derivatives and monitored at m/z 844 and 853. For LC/MS with electrospray ionization, the transitions m/z 652/661 to 606/614 were monitored. For use of the methods as candidate reference methods, special attention was paid to the calibration and the measurement protocol (duplicate analysis of each sample on three occasions). Evaluation of the ID-GC/MS and ID-LC/MS/MS methods showed the absence of interference by reverse T3 and T4, a limit of detection of 100 pg (GC/MS) and 18 pg (LC/MS), a recovery of 100 +/- 1.5% (95% confidence interval) and good precision (the total coefficient of variation, n = 6, was typically 1.5%). In addition to the recovery study, the accuracy of the methods was proven by method comparison (ID-GC/MS vs. LC/MS/MS) on three sera, showing a maximum deviation of 1.1%. Finally, the ID-GC/MS method was applied for measurement of 10 different human sera with a T3 concentration range from 0.6 to 7.3 ng/mL. SN - 0951-4198 UR - https://www.unboundmedicine.com/medline/citation/10487939/Isotope_dilution_gas_chromatography/mass_spectrometry_and_liquid_chromatography/electrospray_ionization_tandem_mass_spectrometry_for_the_determination_of_triiodo_L_thyronine_in_serum_ L2 - https://doi.org/10.1002/(SICI)1097-0231(19991015)13:19<1924::AID-RCM734>3.0.CO;2-U DB - PRIME DP - Unbound Medicine ER -